CN110838398A - Composite soft magnetic material and preparation method thereof - Google Patents

Composite soft magnetic material and preparation method thereof Download PDF

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Publication number
CN110838398A
CN110838398A CN201911120438.2A CN201911120438A CN110838398A CN 110838398 A CN110838398 A CN 110838398A CN 201911120438 A CN201911120438 A CN 201911120438A CN 110838398 A CN110838398 A CN 110838398A
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China
Prior art keywords
powder
soft magnetic
composite soft
magnetic material
material according
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Pending
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CN201911120438.2A
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Chinese (zh)
Inventor
冯双久
倪江利
刘先松
胡锋
阚绪材
杨玉杰
吕庆荣
朱瑞威
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Anhui University
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Anhui University
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Priority to CN201911120438.2A priority Critical patent/CN110838398A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147Alloys characterised by their composition
    • H01F1/153Amorphous metallic alloys, e.g. glassy metals
    • H01F1/15358Making agglomerates therefrom, e.g. by pressing
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0266Moulding; Pressing

Abstract

The invention discloses a composite soft magnetic material and a preparation method thereof, and relates to the technical field of composite soft magnetic materials. The insulating material plays the roles of insulation and adhesive, so that the material is saved, the manufacturing process is simpler, and the compression stability of the compounded material is higher.

Description

Composite soft magnetic material and preparation method thereof
Technical Field
The invention relates to the technical field of soft magnetic materials, in particular to a composite soft magnetic material and a preparation method thereof.
Background
Soft magnetic materials have many applications, such as core materials in inductors, stators and rotors in electrical machines, actuators, sensors and transformer cores.
The soft magnetic composite material is manufactured by adopting a powder metallurgy technology, consists of surface-insulated metal powder particles (such as pure iron powder), can be pressed into a part with a complex shape in one step, has good three-dimensional isotropic magnetic property and lower eddy current loss at medium-high frequency, can be used as an iron core material in motors with complex shapes and magnetic circuits and motors working at higher frequency, and can bring revolutionary change to the design of a power supply motor while being widely applied. With the development of miniaturization and high frequency of electronic devices, micro motors, low-power motors, anti-electromagnetic interference elements and the like are widely applied to automobiles, robots, offices and home automation equipment, and the application of soft magnetic composite materials with unique performance in the fields can generate huge economic benefits.
In the existing production of soft magnetic composite materials, an electric insulating layer is arranged on each particle in an insulating coating mode. The traditional powder metallurgy process is used, the metal magnetic powder and the insulated particles are mixed and pressed together with a lubricant and/or an adhesive optionally, and the existing preparation method of the soft magnetic composite material powder has the disadvantages of complex process, high production cost, low production efficiency, low product quality and difficulty in meeting higher use requirements.
Disclosure of Invention
The present invention is directed to a composite soft magnetic material to solve the problems set forth in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
a composite soft magnetic material is composed of metal magnetic powder and low-melting-point glass powder.
The low-melting-point glass powder accounts for 0.5-10% of the weight of the composite soft magnetic material.
The low-melting-point glass powder accounts for 2 percent of the weight of the composite soft magnetic material.
The metal magnetic powder is Fe, Fe-Ni-Mo, Fe-Si-Cr, Fe-Si-Al metal powder, amorphous and nano crystalline alloy powder or permalloy powder and mixed powder of the amorphous and nano crystalline alloy powder and the permalloy powder.
The main component of the low-melting-point glass powder is lead-free glass powder with the melting point of 300-700 ℃, or B2O3Or H3BO3And (3) pulverizing.
The preparation method of the composite soft magnetic material comprises the steps of taking metal magnetic powder as a raw material, adding the metal magnetic powder and the low-melting-point glass powder, uniformly mixing, wherein the weight percentage of the low-melting-point glass powder in the mixture is 0.5-10%, then adding a release agent accounting for 0.3-1% of the weight percentage of the mixture of the metal magnetic powder and the low-melting-point glass powder, molding the powder into a powder core with the shape of a required product under the pressure of 500 plus materials and 5000MPa, placing the powder core in a vacuum furnace or an atmosphere protection furnace, and carrying out heat treatment at the temperature of 200 plus materials and 700 ℃ for 5 minutes to 5 hours to obtain a finished product of the powder core material.
The release agent is zinc stearate.
The treatment temperature was 500 ℃.
Compared with the prior art, the invention has the following beneficial effects:
compared with the prior art that the insulating material and the metal powder material are solidified and connected into a whole under certain temperature control by adopting an organic adhesive, the insulating material plays the roles of insulation and the adhesive, saves materials and is easier to obtain the powder core material with high saturation magnetization. The manufacturing process is simpler, the aging problem does not exist, and the compression stability of the compounded material is higher.
Drawings
FIG. 1 is a graph showing the loss separation of FeSi powder cores with 2 wt% of low-melting glass powder added according to the present invention;
FIG. 2 shows the addition of 1 wt% B according to the present invention2O3The FeSiCr powder core loss separation diagram.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
spherical FeSi6.5wt% powder with the particle size of 30-100 mu m is used as a raw material, 2 wt% of low-melting-point glass powder is added to be used as an insulating agent and an adhesive to be uniformly mixed, the melting point of the glass powder is 400 ℃, and the average particle size is 5 mu m. 0.5% by weight of zinc stearate was additionally added as a mold release agent, and the powder was molded into an annular powder core having an outer diameter of 27mm, an inner diameter of 15mm and a height of about 8mm under a pressure of 1200 MPa. And (3) placing the FeSi powder core in a vacuum furnace, and carrying out heat treatment at 450 ℃ for 1 hour to obtain a powder core material finished product.
The magnetic measurement result shows that the specific saturation magnetization of the material reaches 203emu/g, the initial permeability is 51, and the loss under 100kHz and 100mT is 2300kW/m3. The power consumption versus frequency measured for this sample over a period is shown in fig. 1, from which it can be seen that the lower slope indicates that the FeSi powder core has relatively less eddy current loss, indicating that low melting glass does perform well for insulation.
Example 2:
commercial FeSiCr powder in the market is taken as a basic raw material, and 1 wt% of B is added2O3The insulating agent and the adhesive are uniformly mixed. 0.5% by weight of zinc stearate was additionally added as a mold release agent, and the powder was pressed under a pressure of 500MPa into an annular powder core having a diameter of 20mm, an inner diameter of 10mm and a height of about 5 mm. And placing the powder core in a nitrogen protection sintering furnace, and performing heat treatment at 500 ℃ for 30 minutes to obtain a powder core material finished product.
The magnetic test shows that the initial magnetic permeability of the powder core is 38, 100kHz, and the loss at 100mT is about 4800kW/m3. FIG. 2 shows the power consumption versus frequency for one cycle measured for this sample, from which it can be seen that the lower slope indicates that the FeSiCr powder core has relatively less eddy current lossConsumption, shows B2O3And a good insulation effect is achieved. The total loss of the powder core is relatively large, but the eddy current loss is relatively low, and is mainly contributed by the hysteresis loss.
Example 3:
adopts the nano-crystalline powder of Antai science and technology, adds 3 wt% of B-Si-P-O glass powder as an insulating agent and an adhesive, and uniformly mixes. 0.5% by weight of zinc stearate was additionally added as a mold release agent, and the mixed powder was pressed under a pressure of 700MPa into an annular powder core having an outer diameter of 20mm, an inner diameter of 10mm and a height of about 5 mm. Heat treatment in vacuum at 600 ℃ for 30 minutes. Obtaining the nanocrystalline powder core material.
Magnetic measurement shows that the magnetic permeability of the nanocrystalline powder core is 18, and the power consumption at 100kHz and 100mT is 2100kW/m3. The nanocrystalline powder core has the greatest advantage of being applicable to MHz frequency bands. However, the fine powder has a certain slag falling phenomenon. Increasing the heat treatment temperature may improve the slag removal problem, but the magnetic properties may deteriorate rapidly.
Example 4:
adopts the nano-crystalline powder of Antai science and technology, and is added with 10wt percent of H3BO3The insulating agent and the adhesive are uniformly mixed. 0.5% by weight of zinc stearate was additionally added as a mold release agent, and the mixed powder was pressed under a pressure of 5000MPa into a ring-shaped powder core having an outer diameter of 10mm, an inner diameter of 6mm and a height of about 4 mm. Heat treatment in vacuum at 700 ℃ for 5 minutes. Obtaining the nanocrystalline powder core material.
Magnetic measurement shows that the magnetic permeability of the nanocrystalline powder core is 8, and the power consumption under 100kHz and 30mT is 2500kW/m3. The nanocrystalline powder has no slag falling phenomenon, but the magnetic relaxation frequency is reduced to about 600kHz, and the saturation magnetization intensity is also lower.
Example 5:
spherical high-purity Fe powder with the average grain diameter of 50 mu m is taken as a raw material, 0.5 wt% of low-melting-point glass powder is added to be taken as an insulating agent and a bonding agent to be uniformly mixed, and the average grain diameter of the glass powder is 3 mu m. 0.5% by weight of zinc stearate was additionally added as a mold release agent, and the powder was molded into an annular powder core having an outer diameter of 21mm, an inner diameter of 15mm and a height of about 6mm under a pressure of 2000 MPa. And placing the powder core in a vacuum furnace, and carrying out heat treatment at 200 ℃ for 5 hours to obtain a powder core material finished product.
The magnetic measurement result shows that the specific saturation magnetization of the material reaches 211emu/g, the initial permeability is 42, and the loss under 100kHz and 100mT is 4700kW/m3. The low-temperature heat treatment is advantageous for improving the frequency stability of the magnetic properties, but a high-strength powder core cannot be obtained.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (8)

1. The composite soft magnetic material is characterized by consisting of metal magnetic powder and low-melting-point glass powder.
2. A composite soft magnetic material according to claim 1, characterized in that the low melting point glass powder accounts for 0.5-10% by weight of the composite soft magnetic material.
3. A composite soft magnetic material according to claim 2, characterised in that the low melting glass frit is present in an amount of 2% by weight of the composite soft magnetic material.
4. A composite soft magnetic material according to claim 1 or 2, characterized in that the metallic magnetic powder is Fe, Fe-Ni-Mo, Fe-Si-Cr, Fe-Si-Al metal powder, amorphous, nanocrystalline alloy powder or permalloy powder and mixed powder therebetween.
5. A composite soft magnetic material according to claim 1 or 2, characterized in that the low melting point glass frit mainly comprises a lead-free glass frit having a melting point of 300-700 ℃, or B2O3Or H3BO3And (3) pulverizing.
6. The method for preparing the composite soft magnetic material according to any one of claims 1 to 3, characterized in that the metal magnetic powder is used as a raw material, the metal magnetic powder and the low melting point glass powder are added and mixed uniformly, wherein the weight percentage of the low melting point glass powder in the mixture is 0.5 to 10%, the release agent with the weight percentage of 0.3 to 1% is added in the mixture of the metal magnetic powder and the low melting point glass powder, the powder is molded into a powder core with a desired product shape under the pressure of 500 plus 5000MPa, the powder core is placed in a vacuum furnace or an atmosphere protection furnace, and the powder core material finished product is obtained after heat treatment at 200 plus 700 ℃ for 5 minutes to 5 hours.
7. The method for preparing a composite soft magnetic material according to claim 6, wherein the release agent is zinc stearate.
8. A method for the production of a composite soft magnetic material according to claim 6, characterised in that the treatment temperature is 500 ℃.
CN201911120438.2A 2019-11-15 2019-11-15 Composite soft magnetic material and preparation method thereof Pending CN110838398A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006278833A (en) * 2005-03-30 2006-10-12 Mitsubishi Materials Pmg Corp Manufacturing method of composite soft-magnetic sintered material having high strength, high magnetic-flux density, and high resistance
JP2010238914A (en) * 2009-03-31 2010-10-21 Mitsubishi Materials Corp Method of producing high strength low loss composite soft magnetic material, and high strength low loss composite soft magnetic material
JP2018198281A (en) * 2017-05-24 2018-12-13 Tdk株式会社 Iron nitride magnet
CN109036753A (en) * 2018-07-02 2018-12-18 四川大学 A kind of amorphous nano-crystalline composite magnetic powder core and preparation method thereof
CN109585115A (en) * 2017-09-29 2019-04-05 精工爱普生株式会社 Insulant coats soft magnetic powder, compressed-core, magnetic element, electronic equipment

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006278833A (en) * 2005-03-30 2006-10-12 Mitsubishi Materials Pmg Corp Manufacturing method of composite soft-magnetic sintered material having high strength, high magnetic-flux density, and high resistance
JP2010238914A (en) * 2009-03-31 2010-10-21 Mitsubishi Materials Corp Method of producing high strength low loss composite soft magnetic material, and high strength low loss composite soft magnetic material
JP2018198281A (en) * 2017-05-24 2018-12-13 Tdk株式会社 Iron nitride magnet
CN109585115A (en) * 2017-09-29 2019-04-05 精工爱普生株式会社 Insulant coats soft magnetic powder, compressed-core, magnetic element, electronic equipment
CN109036753A (en) * 2018-07-02 2018-12-18 四川大学 A kind of amorphous nano-crystalline composite magnetic powder core and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张达理等: "低熔点玻璃粉包覆FeSiAl合金的结构和电磁性能", 《材料研究学报》 *

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